CN115198111A - Lithium extraction method for lithium-containing waste aluminum electrolyte - Google Patents
Lithium extraction method for lithium-containing waste aluminum electrolyte Download PDFInfo
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- CN115198111A CN115198111A CN202210852836.9A CN202210852836A CN115198111A CN 115198111 A CN115198111 A CN 115198111A CN 202210852836 A CN202210852836 A CN 202210852836A CN 115198111 A CN115198111 A CN 115198111A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
- C22B26/12—Obtaining lithium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/08—Carbonates; Bicarbonates
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention relates to a lithium extraction method of lithium-containing waste aluminum electrolyte, which comprises the following steps: crushing the lithium-containing waste aluminum electrolyte to be treated to obtain electrolyte powder; uniformly mixing the electrolyte powder and a reactant, roasting at 600-1400 ℃ for 0.5-5h, cooling, and grinding to obtain mixture powder; mixing the mixture powder with water, stirring for reaction, and filtering to obtain filter residue and filtrate; and (4) using the filtrate for lithium precipitation to obtain a lithium salt. The whole treatment process of the invention does not use acid or alkali, the reactants are cheap and easy to obtain, the production process is environment-friendly, and the working condition is friendly. The roasting-water leaching lithium extraction process has the advantages of short process flow, simple equipment and high industrial feasibility.
Description
Technical Field
The invention relates to a lithium extraction method of lithium-containing waste aluminum electrolyte, belonging to the field of metallurgical solid waste recycling treatment.
Background
With the rapid development of new energy industry, in recent years, the price of battery-grade lithium carbonate rises from 3-5 ten thousand per ton to 50 ten thousand per ton, and lithium extraction becomes a research hotspot in various fields. During the process of aluminum electrolysis, lithium (reduced to Li) is contained in low-grade bauxite 2 O>0.58%) was continuously enriched in the cell with the alumina feed, resulting in a gradual increase in the lithium content of the electrolyte. For example, in some areas, the electrolyte of an aluminum electrolysis plant contains up to 1 to 3% Li in terms of Li 2 The O content is 2.1-6.4%, which is close to 1.5-7% of the spodumene ore, and the lithium extraction value is high. Therefore, the lithium-containing waste electrolyte generated in the electrolytic process of the aluminum plant becomes an important lithium extraction resource.
Phase analysis shows that lithium in the waste electrolyte containing lithium is mainly Na 2 LiAlF 6 The form exists, not the traditionally recognized LiF, due to the molecular ratio of aluminum electrolyte ([ NaF ]) in China]/[AlF 3 ]) 1.8-2.6, and is an acid electrolyte in which lithium electrode is easily combined with excess aluminum fluoride to form Na 2 LiAlF 6 . However, na 2 LiAlF 6 Has the same effect as Na 3 AlF 6 Similar in nature, poorly soluble in water, which increases the difficulty of extracting lithium from spent electrolytes.
Chinese patent CN 109930174B discloses a method for removing lithium, purifying and recovering lithium from aluminum electrolyte, and proposes to use 2-6mol/L HNO at 40-120 DEG C 3 Leaching waste electrolyte containing lithium for 0.5-10h, leaching lithium into the solution, filtering to obtain filtrate, evaporating to lithium concentration of 3-8g/L, naturally cooling and crystallizing to obtain NaNO 3 Then adjusting the pH value to 6-7, and continuing natural cooling to obtain secondary NaNO 3 Sequentially adding calcium salt and oxalic acid into the filtrate for purification and impurity removal, and adding alkaline substances according to needs for precipitation to obtain Li 2 CO 3 Or (and) LiOH. The process realizes the extraction of lithium from waste electrolyte, but uses HNO 3 It reacts with fluorine in the electrolyte to generate a large amount of HF, which not only corrodes equipment, but also causes environmental pollution, endangering the life and health of operators. China invention patent application CN 108569711A proposes miningHeating and leaching 5-8% sulfuric acid at 90-95 deg.C for 0.5-1.5 hr to obtain lithium sulfate solution, removing impurities from the obtained leachate, evaporating, concentrating and precipitating lithium, and the process still uses strong acid and has HF problem.
In order to reduce the acid dosage, researchers have proposed pre-treating the lithium-containing electrolyte with Na 2 LiAlF 6 Converted to LiF, which is easily leached. For example, the Chinese patent application CN 105543504A proposes adding sodium fluoride into lithium-containing aluminum electrolyte, mixing uniformly, and keeping the temperature at 400-100 deg.C for 2-3h to make Na 2 LiAlF 6 The conversion is easy to leach LiF, but 7-14mol/L of strong acid is still used for leaching, so that the defect that HF is generated by strong acid leaching cannot be overcome.
For this purpose, the Chinese patent application CN 112919507A proposes to use 2.5-5mol/L sodium hydroxide solution to leach the electrolyte at 80-100 ℃ so that Na in the electrolyte is obtained 2 LiAlF 6 And (4) converting the Li into LiF, wherein the LiF exists in the filter residue, and the filter residue is leached at 50-90 ℃ by using 1-4mol/L acid to dissolve out the Li. Clearly, the process reduces the acid concentration and HF volatilization, but still does not solve the problem radically. In addition, the used strong alkali liquor can corrode an iron-based metal container at 80-100 ℃ to cause alkali brittleness, only nickel-based materials can resist strong alkali corrosion at high temperature, and single nickel materials are high in price which is dozens of times of steel, so that the equipment investment is increased undoubtedly.
Chinese patent application CN110284157A discloses a method for recycling anode carbon slag and aluminum electrolyte, which comprises: uniformly mixing anode carbon residue and/or aluminum electrolyte with a calcium-containing substance and an alkali-containing substance to form a mixture, and crushing and grinding the mixture; roasting the ground mixture at a preset temperature for a preset time; grinding the roasted product, then heating, stirring and leaching the ground roasted product in an alkali-containing solution, and filtering the leached slurry; washing and drying the filter residue to obtain calcium fluoride; the filtrate is sodium aluminate solution, the main components of which are caustic alkali and sodium aluminate, and the filtrate can be directly returned to the process of producing alumina by the Bayer process for utilization. The method not only needs to add alkali for roasting, but also needs to add alkali for leaching, and the alkali consumption is larger.
Therefore, the lithium extraction from the waste electrolyte leached by strong acid and strong base has corresponding disadvantages, particularly the problems of equipment corrosion and environmental protection caused by HF generated by strong acid treatment severely restrict the industrial application of the electrolyte. Therefore, it is important to develop a lithium extraction process for non-acid and non-alkali electrolyte.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide a lithium extraction method of lithium-containing waste aluminum electrolyte without consuming acid and alkali.
In order to solve the technical problems, the technical scheme of the invention is as follows:
a method for extracting lithium from lithium-containing waste aluminum electrolyte comprises the following steps:
s1, crushing lithium-containing waste aluminum electrolyte to be treated to obtain electrolyte powder;
s2, uniformly mixing the electrolyte powder with a reactant, roasting at 600-1400 ℃ for 0.5-5h, cooling, and grinding to obtain mixture powder;
wherein the reactant is MgCl 2 、CaCl 2 、BaCl 2 、Mg(NO 3 ) 2 、Ca(NO 3 ) 2 、Ba(NO 3 ) 2 、MgSO 4 、CaSO 4 、BaSO 4 And hydrates thereof;
s3, mixing the mixture powder with water, stirring for reaction, and filtering to obtain filter residues and a filtrate;
and S4, using the filtrate for lithium precipitation to obtain lithium salt.
Further, in S1, the particle size of the electrolyte powder is less than or equal to 0.5mm, more specifically, less than 0.3mm, preferably, less than 0.15mm, and more preferably, less than or equal to 0.1mm.
Further, in the lithium-containing waste aluminum electrolyte, lithium exists in the form of Na 2 LiAlF 6 And/or LiF. Further, lithium is mainly represented by Na 2 LiAlF 6 Is present and secondly is present in the form of LiF.
Further, the lithium-containing waste aluminum electrolyte includes Na 3 AlF 6 25-80％、Na 2 LiAlF 6 8-70％、Na 2 KAlF 6 0-30％、Al 2 O 3 0-5％、CaF 2 0-6％、MgF 2 0-2％、LiF0-5％。
Further, the lithium-containing waste aluminum electrolyte includes Na 3 AlF 6 30-75％、Na 2 LiAlF 6 12-65％、Na 2 KAlF 6 5-25％、Al 2 O 3 1-4％、CaF 2 1-5％、MgF 2 0.5-1.5％、LiF1-4％。
In S2, the ratio of the mole number of the reactant to the mole number of aluminum in the electrolyte powder is 2 to 6, further 2.5 to 4.
Furthermore, in S2, the roasting temperature is 850-1100 ℃, and the roasting time is 1-4.5h, preferably 1-2h.
Further, in S3, the solid-liquid mass-volume ratio of the mixture powder to water is 1g to 10mL, preferably 1 g.
Further, in S3, the reaction time is stirred for 0.1 to 5 hours, further 0.5 to 3.5 hours, preferably 1 to 3 hours.
Further, in S3, the reaction temperature is 20 to 100 ℃, preferably 50 to 95 ℃, and more preferably 80 to 90 ℃.
Optionally, a step of removing impurities from the filtrate is further included between S3 and S4, that is, an impurity removing agent is added into the filtrate to remove residual calcium and fluorine ions; preferably, the impurity removing agent comprises Na 2 CO 3 、K 2 CO 3 At least one of activated alumina and EDTA. Optionally, after adding the impurity removing agent, stirring and reacting for 10-180min, preferably, the reaction time is 20-50min. Optionally, the reaction temperature is controlled to be 20-100 ℃ and preferably 40-60 ℃ during impurity removal.
Further, in S4, lithium is extracted from the filtrate with reference to the prior art.
Further, in S4, water-soluble carbonate or a solution thereof is added to the filtrate, and lithium is precipitated to obtain lithium carbonate.
In the invention, na in the lithium-containing waste electrolyte can be made by the roasting treatment of S2 2 LiAlF 6 Or/andlithium of LiF is converted into easily soluble lithium salt, such as LiCl, li 2 SO 4 、LiNO 3 F and Al form CaF 2 And Al 2 O 3 Insoluble matter, leaching Li into solution by water leaching of S3, and CaF 2 And Al 2 O 3 The lithium is kept in a slag phase, so that the separation of lithium from aluminum, calcium and the like is realized; the filter residue can be further used as hydrofluoric acid production raw material. In addition, the added reactant can play a role in fixing fluorine in the roasting process, so that the possibility of fluoride volatilization is effectively reduced, and the roasting process is more environment-friendly compared with the roasting process of the prior art such as CN 201510970561.9.
Compared with the prior art, the invention has the following beneficial effects:
(1) The whole treatment process does not use acid and alkali, the used reactants are sulfate, hydrochloride and nitrate of calcium, magnesium and barium, the reactants are cheap and easy to obtain, the production process is environment-friendly, and the working condition is friendly.
(2) The roasting-water leaching lithium extraction process has the advantages of short process flow, simple equipment and high industrial feasibility.
Drawings
Fig. 1 is an XRD spectrum of the lithium-containing waste electrolyte used in example 1.
FIG. 2 is an XRD pattern of the mixture after calcination reaction of example 1.
Fig. 3 is an XRD pattern of lithium carbonate obtained in example 1.
FIG. 4 is the XRD pattern of the mixture after calcination reaction of example 2.
Detailed Description
The present invention will be described in detail with reference to examples. It should be noted that the embodiments and features of the embodiments of the present invention may be combined with each other without conflict.
Example 1
The specific implementation steps of this embodiment are as follows:
(1) 100g (Na) of lithium-containing waste aluminum electrolyte from Qinghai certain factory 3 AlF 6 38.5％、Na 2 LiAlF 6 33.5％、Na 2 KAlF 6 17.6％、Al 2 O 3 5.8％、CaF 2 2.8％、MgF 2 1.0%), and a phase analysis spectrum thereof is shown in figure 1, and electrolyte powder with the grain diameter less than or equal to 0.15mm is obtained by crushing and grinding;
(2) Adding calcium chloride into 100g of electrolyte powder to ensure that the molar ratio of the calcium chloride to aluminum elements in the electrolyte powder is 3.3;
(3) Adding deionized water into the mixture to ensure that the liquid-solid ratio is 1g (4 mL), reacting for 1h at 70 ℃ under the stirring of 500rpm, and filtering to obtain filter residue and filtrate;
(4) Adding 0.5g of sodium carbonate powder into the filtrate, stirring and reacting at normal temperature for 20min, and filtering to obtain filtrate a;
(5) Evaporating and concentrating the filtrate a until the mass concentration of lithium is 20g/L, filtering, adding 10g of sodium carbonate into the filtrate at 95 ℃, stirring and reacting for 1h, then aging for 2h at 95 ℃, filtering while hot at high temperature, washing the filter cake twice with 30ml of deionized water, filtering, and drying to obtain 4.5g of lithium carbonate;
FIG. 2 is an XRD pattern of the calcined product obtained in step (2), and it can be seen that Na is not contained in the phase 2 LiAlF 6 Peaks, indicating complete reaction of the phase; na (Na) 3 AlF 6 Only a very weak peak remains, indicating that most of the reaction is consumed; the product generated by the reaction is CaF 2 NaCl and Al 2 O 3 The diffraction peak is obvious and is a main phase; the product LiCl was low in content, and no diffraction peak was directly observed.
And (3) detecting and analyzing the obtained lithium carbonate, taking three groups of samples, wherein each group is 0.3g, dissolving the samples by using hydrochloric acid, and then carrying out ICP detection to obtain the product, wherein the purity of the lithium carbonate is 98.1%, and an XRD (X-ray diffraction) spectrum of the lithium carbonate is shown in figure 3. The lithium leaching rate in step (3) was calculated to be 90.2%.
Example 2
Example 1 was repeated with the only difference that: in the step (2), calcium chloride is changed into calcium sulfate. The XRD pattern of the calcined product is shown in figure 4, and the purity of the obtained lithium carbonate product is 98.6%. The leaching rate of lithium was 91.0%.
Example 3
Example 1 was repeated with the only difference that: in the step (2), the calcium chloride is changed into magnesium chloride. The purity of the obtained lithium carbonate product is 97.5%.
The leaching rate of lithium was 89.8%.
Example 4
Example 1 was repeated with the only difference that: in the step (2), the calcium chloride is changed into barium chloride. The purity of the obtained lithium carbonate product is 97.9%.
The leaching rate of lithium was 92.1%.
Example 5
Example 1 was repeated with the only difference that: in the step (2), the calcination temperature was changed to 800 ℃. The purity of the obtained lithium carbonate product is 97.3 percent.
The leaching rate of lithium was 81.6%.
Example 6
Example 1 was repeated with the only difference that: in the step (2), the calcination temperature was changed to 900 ℃. The purity of the obtained lithium carbonate product is 97.3 percent.
The leaching rate of lithium was 86.8%.
Example 7
Example 1 was repeated with the only difference that: in the step (2), the molar ratio of calcium chloride to aluminum element in the electrolyte powder is 2.2.
The purity of the obtained lithium carbonate product is 97.4%. The leaching rate of lithium was 58.6%.
Example 8
Example 1 was repeated with the only difference that: in the step (2), the molar ratio of calcium chloride to aluminum element in the electrolyte powder is 2.8.
The purity of the obtained lithium carbonate product is 97.4%. The leaching rate of lithium was 79.6%.
The foregoing examples are set forth to illustrate the present invention more clearly and are not to be construed as limiting the scope of the invention, which is defined in the appended claims to which the invention pertains, as modified in all equivalent forms, by those skilled in the art after reading the present invention.
Claims (8)
1. A method for extracting lithium from lithium-containing waste aluminum electrolyte is characterized by comprising the following steps:
s1, crushing lithium-containing waste aluminum electrolyte to be treated to obtain electrolyte powder;
s2, uniformly mixing the electrolyte powder and a reactant, roasting at 600-1400 ℃ for 0.5-5h, cooling, and grinding to obtain mixture powder;
wherein the reactant is MgCl 2 、CaCl 2 、BaCl 2 、Mg(NO 3 ) 2 、Ca(NO 3 ) 2 、Ba(NO 3 ) 2 、MgSO 4 、CaSO 4 、BaSO 4 And hydrates thereof;
s3, mixing the mixture powder with water, stirring for reaction, and filtering to obtain filter residues and a filtrate;
and S4, using the filtrate for lithium precipitation to obtain lithium salt.
2. The method for extracting lithium from lithium-containing waste aluminum electrolyte according to claim 1, wherein the particle size of the electrolyte powder in S1 is less than or equal to 0.5mm, preferably less than or equal to 0.1mm.
3. The method for extracting lithium from lithium-containing waste aluminum electrolyte according to claim 1, wherein the molar ratio of the reactant to aluminum in the electrolyte powder in S2 is 2-6, preferably 2.5-4.
4. The method for extracting lithium from lithium-containing waste aluminum electrolyte according to claim 1, wherein in S2, the roasting temperature is 850-1100 ℃, and the roasting time is 1-4.5h, preferably 1-2h.
5. The method for extracting lithium from lithium-containing waste aluminum electrolyte according to claim 1, wherein in S3, the solid-liquid volume ratio of the mixture powder to water is 1g to 10mL, preferably 1g to 4mL.
6. The method for extracting lithium from lithium-containing waste aluminum electrolyte according to claim 1, wherein the stirring reaction time in S3 is 0.1-5h, further 0.5-3.5h, preferably 1-3h.
7. The method for extracting lithium from lithium-containing waste aluminum electrolyte according to claim 1, wherein the reaction temperature in S3 is 20-100 ℃, preferably 50-95 ℃, and more preferably 80-90 ℃.
8. The method of claim 1, wherein in step S4, water-soluble carbonate or a solution thereof is added to the filtrate to precipitate lithium, thereby obtaining lithium carbonate.
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Cited By (2)
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| CN116334411A (en) * | 2023-04-11 | 2023-06-27 | 珠海市瑞斐门特科技有限公司 | Recovery method for extracting lithium element from aluminum electrolyte slag at low temperature in multiple stages |
| CN117327923A (en) * | 2023-10-18 | 2024-01-02 | 河南新天力循环科技有限公司 | Method for jointly extracting lithium from waste aluminum electrolyte and overhaul slag |
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